BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF GEMIGLIPTIN TARTRATE SESQUIHYDRATE.
Shailesh V. Luhar*, Harshi A. Patel, Dr. G. K. Jani and Dr. P. Malairajan
ABSTRACT
A simple, selective, specific, accurate Liquid Chromatography -Mass Spectrometry (LC-MS) method was developed and validated for the determination of Gemigliptin in Human Plasma. The accuracy and precision data must fulfill the requirements for the quantification of analytes in biological matrices to produce data for bioavailability, bioequivalence, etc. The separation of the analyte was carried out on Phenomenex Gemini C18 , (3 μm, 30.0 × 2.0 mm) column and the mobile phase containing 0.1% Formic acid in 10 mM Ammonium acetate in water : Acetonitrile (10:90% v/v) at a flow rate of 0.5 mL/min. The retention times of Gemigliptin and Sitagliptin (Internal Standard) were 3.29 min and 4.22 min simultaneously and the total run time was 5.5 min. Monitoring of the fragmentation of m / z 490.160 → 338.100 and 408.142 → 235.000 performed during MS/MS detection of Gemigliptin and Internal Standard (I.S.) on the mass spectrometer. The overall recovery of Gemigliptin and IS was 89.81% and 89.52% respectively. The method was validated over the concentration range of 1 ng/mL to 2000 ng/mL. The method was validated for linearity, accuracy, precision, specificity, selectivity, inter and intraday precision, LQC, HQC.
Keywords: Gemigliptin, LC-MS, Bioanalytical Method, validation.
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